CN105218827B - A kind of organic group modification super high molecular weight polysiloxanes and preparation method thereof - Google Patents
A kind of organic group modification super high molecular weight polysiloxanes and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of organic group modification super high molecular weight polysiloxanes, its structural formula such as formula (1) are shown.The invention also discloses the preparation method of the organic group modification super high molecular weight polysiloxanes.The present invention can prepare the organic group modification super high molecular weight polysiloxanes of molecular weight more than 1,000,000, the present invention among super high molecular weight polysiloxane molecule chain by being grafted long-chain alkyl-silicone oil molecule, add the physical blending compatibility with polyolefin, simultaneously unsaturated double-bond is introduced at chain both ends, reactive grafting can be carried out with polyolefin, further increase is chemical binding with polyolefin, so as to substantially increase the mechanical property of polyolefin, scraping and wiping resistance performance and heat resistance.
Description
Technical field：
The present invention relates to the technical field of modification of super high molecular weight polysiloxanes, is specifically related to a kind of organic group modification
Super high molecular weight polysiloxanes.
Background technology：
Super high molecular weight polysiloxanes has the advantages of pliability is good, heat resistance and scraping and wiping resistance performance are good, but its with
The solubility parameter difference of polyolefin is larger, therefore both compatibilities are poor.In order that super high molecular weight polysiloxanes and polyene
Hydrocarbon can be combined together well, it is necessary to increase both compatibilities.The present invention is by among the chain of polysiloxane molecule chain
Long-chain alkyl-silicone oil molecule is grafted, so as to improve its physical blending compatibility with polyolefin, is introduced not at the both ends of strand
Saturation double bond, control the molecular weight of polysiloxanes for 1,000,000 and more than, reach the degree of super high molecular weight, utilize end active group
Group and polyolefin reactive grafting, increase it is chemical binding with polyolefin, so as to substantially increase the mechanical property of polyolefin, resistance to
Scratch performance and heat resistance.
The content of the invention：
It is an object of the invention to provide a kind of organic group modification super high molecular weight polysiloxanes, and it is compatible with polyolefin
Property is good, can effectively improve mechanical property, scraping and wiping resistance performance and the heat resistance of polyolefin.
It is a further object to provide the preparation method of the organic group modification super high molecular weight polysiloxanes.
To achieve the above object, the present invention uses following technical scheme：
A kind of organic group modification super high molecular weight polysiloxanes, shown in its structural formula such as formula (1)：
In formula (1), a+b sums are the integer more than 12000, and c+d+e sums are 15~250 integer, and f is 6~16
Integer, R is one kind in formula (2), formula (3), formula (4) and formula (5), as follows：
A kind of preparation method of organic group modification super high molecular weight polysiloxanes, comprises the following steps：
(1) long-chain alpha-olefin activity platinum catalyst is prepared
By the alcoholic solution of long-chain alpha-olefin and chloroplatinic acid in 60~80 DEG C of 2~6h of priming reaction, then it is evaporated under reduced pressure 2~
4h, obtain long-chain alpha-olefin activity platinum catalyst；
(2) chain alkyl containing hydrogen silicone oil is prepared
By the long-chain alpha-olefin activity platinum catalyst obtained by step (1) and containing hydrogen silicone oil, long-chain alpha-olefin in 80~120
DEG C 2~6h of reaction, then heats to 140~180 DEG C, is evaporated under reduced pressure 2~4h, obtains that there is the chain alkyl of formula (6) structure to contain
Hydrogen silicone oil,
In formula (6), c+d+e sums are 15~250 integer, and f is 6~16 integer；
(3) methylvinylcyclosiloxane activity platinum catalyst is prepared
By the alcoholic solution of methylvinylcyclosiloxane monomer and chloroplatinic acid in 60~80 DEG C of 2~6h of priming reaction, then
2~4h is evaporated under reduced pressure, obtains methylvinylcyclosiloxane activity platinum catalyst；
(4) long-chain alkyl-silicone oil grafting cyclosiloxane is prepared
By obtained by the chain alkyl containing hydrogen silicone oil obtained by methylvinylcyclosiloxane monomer, step (2) and step (3)
The methylvinylcyclosiloxane activity platinum catalyst arrived reacts 2~6h in 80~120 DEG C, then rises to 140~180 DEG C of decompressions
2~4h is distilled, obtains the long-chain alkyl-silicone oil grafting cyclosiloxane with formula (7) structure,
In formula (7), c+d+e sums are 15~250 integer, and f is 6~16 integer, and g is 3~5 integer；
(5) organic group modification super high molecular weight polysiloxanes is prepared
By obtained by cyclosiloxane monomer, step (4) long-chain alkyl-silicone oil grafting cyclosiloxane and catalyst alkali glue in
40~70 DEG C of 0.5~2h of vacuum distillation, then add unsaturated double-bond end-capping reagent in 60~80 DEG C, then rise to 90~130 DEG C
1~4h is reacted, 140~220 DEG C of 4~8h of vacuum distillation is then risen to, produces the organic group modification superelevation with formula (1) structure
Molecular weight silicone.
As the preferred of above-mentioned technical proposal, long-chain alpha-olefin described in step (1) be 1- octenes, 1- nonenes, 1- decene,
1- hendecenes, 1- laurylenes, 1-tetradecylene, 1- hexadecylenes and 1- octadecylenes one of which or several.
As the preferred of above-mentioned technical proposal, the platinum content described in step (1) in the alcoholic solution of chloroplatinic acid is 0.1%,
And alcohol used is absolute ethyl alcohol or isopropanol.
As the preferred of above-mentioned technical proposal, the quality of the alcoholic solution of long-chain alpha-olefin and chloroplatinic acid described in step (1)
Than for 1:0.01~0.2.
As the preferred of above-mentioned technical proposal, the hydrogen content of containing hydrogen silicone oil described in step (2) is 0.1~1.6%.
As the preferred of above-mentioned technical proposal, containing hydrogen silicone oil described in step (2) and long-chain alpha-olefin are by si-h bond and double
Key mol ratio is 1:0.5~1.2 is reacted.
As the preferred of above-mentioned technical proposal, described in step (2) in long-chain alpha-olefin activity platinum catalyst platinum content
For the 0.0001%~0.005% of containing hydrogen silicone oil, long-chain alpha-olefin and long-chain alpha-olefin active platinum catalyst quality summation.
As the preferred of above-mentioned technical proposal, methylvinylcyclosiloxane monomer described in step (3) is trimethyl three
One kind in vinyl cyclotrisiloxane, t etram-ethyltetravinylcyclotetrasiloxane and the vinyl D5 of pentamethyl five.
As the preferred of above-mentioned technical proposal, methylvinylcyclosiloxane monomer used and long alkane in step (4)
Base containing hydrogen silicone oil is 1.1~2 by si-h bond and double bond mol ratio:1 is reacted.
As the preferred of above-mentioned technical proposal, described in step (4) in methylvinylcyclosiloxane activity platinum catalyst
The content of platinum is that methylvinylcyclosiloxane monomer, chain alkyl containing hydrogen silicone oil and methylvinylcyclosiloxane active platinum are urged
The 0.00005%~0.002% of agent quality summation.
As the preferred of above-mentioned technical proposal, cyclosiloxane monomer described in step (5) is hexamethyl cyclotrisiloxane, three
Methyl triphenyl cyclotrisiloxane, octamethylcy-clotetrasiloxane, tetramethyl tetraphenyl cyclotetrasiloxane, decamethylcyclopentaandoxane
With one kind in dimethyl siloxane mixed methylcyclosiloxane.
As the preferred of above-mentioned technical proposal, cyclosiloxane monomer described in step (5) and long-chain alkyl-silicone oil grafting ring
The mass ratio of siloxanes is 1:0.01~1.
As the preferred of above-mentioned technical proposal, catalyst alkali glue described in step (5) is cyclosiloxane monomer and tetramethyl
Ammonium hydroxide is evaporated under reduced pressure in 50~70 DEG C obtained by 4~8h, and wherein the quality of TMAH is cyclosiloxane monomer, length
Alkyl group silicone oil is grafted the 0.002%~0.02% of cyclosilane and catalyst alkali glue gross mass.
As the preferred of above-mentioned technical proposal, unsaturated double-bond end-capping reagent described in step (5) is dimethyl tetravinyl
Disiloxane, tetramethyl divinyl disiloxane, dimethyl tetraallyl disiloxane and the silica of tetramethyl diallyl two
One kind in alkane, and its addition is cyclosiloxane monomer, long-chain alkyl-silicone oil grafting cyclosiloxane and catalyst alkali colloid amount
The 0.01%~0.2% of summation.
Compared with prior art, the invention has the advantages that：
The present invention is added by being grafted long-chain alkyl-silicone oil molecule among the chain of super high molecular weight silicone molecules chain
With the physical blending compatibility of polyolefin, chain both ends introduce unsaturated double-bond, can carry out reactive grafting with polyolefin, add
It is chemical binding with polyolefin, so as to substantially increase the mechanical property of polyolefin, scraping and wiping resistance performance and heat resistance.
Embodiment：
In order to be better understood from the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solving
The present invention is released, any restriction will not be formed to the present invention.
Embodiment 1
A kind of preparation method of organic group modification super high molecular weight polysiloxanes, comprises the following steps：
(1) long-chain alpha-olefin activity platinum catalyst is prepared
It is 1 in mass ratio by the ethanol solution of 1-tetradecylene and chloroplatinic acid:0.05 in 70 DEG C of priming reaction 4h, then
2h is evaporated under reduced pressure, obtains long-chain alpha-olefin activity platinum catalyst；
(2) chain alkyl containing hydrogen silicone oil is prepared
It is 1 that containing hydrogen silicone oil and 1-tetradecylene are pressed into si-h bond and double bond mol ratio:0.8 and platinum content account for gross mass and be
Long-chain alpha-olefin activity platinum catalyst obtained by 0.0003% the step of (1) reacts 3h in 110 DEG C, then rises to 160 DEG C and subtracts
Pressure distillation 2h, obtains the chain alkyl containing hydrogen silicone oil with formula (6) structure；
(3) methylvinylcyclosiloxane active catalyst is prepared
It is 1 in mass ratio by the ethanol solution of t etram-ethyltetravinylcyclotetrasiloxane and chloroplatinic acid:0.05 in 70
DEG C priming reaction 4h, is then evaporated under reduced pressure 2h, obtains methylvinylcyclosiloxane active catalyst；
(4) long-chain alkyl-silicone oil grafting cyclosiloxane is prepared
By the chain alkyl containing hydrogen silicone oil obtained by t etram-ethyltetravinylcyclotetrasiloxane and step (2) by si-h bond and
Double bond mol ratio is 1.1:1 and platinum content account for gross mass for 0.0006% the step of (3) obtained by ethylene methacrylic basic ring silica
Alkane active catalyst reacts 4h in 100 DEG C, then rises to 180 DEG C of vacuum distillation 4h, obtains the chain alkyl with formula (7) structure
Silicone oil is grafted cyclosiloxane；
(5) organic group modification super high molecular weight polysiloxanes is prepared
By the long-chain alkyl-silicone oil grafting cyclosiloxane and tetramethyl hydrogen obtained by octamethylcy-clotetrasiloxane, step (4)
The catalyst alkali glue that amine-oxides content is 1.1% is respectively 100 parts, 20 parts and 0.02 part by mass parts and is evaporated under reduced pressure in 55 DEG C
2h, 0.025 mass parts tetramethyl divinyl disiloxane then is added in 70 DEG C, then rise to 100 DEG C of reactions 1h, Ran Housheng
To 180 DEG C of vacuum distillation 6h, the organic group modification super high molecular weight polysiloxanes with formula (1) structure is produced.
Embodiment 2
A kind of preparation method of organic group modification super high molecular weight polysiloxanes, comprises the following steps：
(1) long-chain alpha-olefin activity platinum catalyst is prepared
It is 1 in mass ratio by the ethanol solution of 1-tetradecylene and chloroplatinic acid:0.05 in 70 DEG C of priming reaction 4h, then
2h is evaporated under reduced pressure, obtains long-chain alpha-olefin activity platinum catalyst；
(2) chain alkyl containing hydrogen silicone oil is prepared
It is 1 that containing hydrogen silicone oil and 1-tetradecylene are pressed into si-h bond and double bond mol ratio:1 and platinum content account for gross mass and be
Long-chain alpha-olefin activity platinum catalyst obtained by 0.0003% the step of (1) reacts 3h in 110 DEG C, then rises to 160 DEG C and subtracts
Pressure distillation 2h, obtains the chain alkyl containing hydrogen silicone oil with formula (6) structure；
(3) methylvinylcyclosiloxane active catalyst is prepared
It is 1 in mass ratio by the ethanol solution of t etram-ethyltetravinylcyclotetrasiloxane and chloroplatinic acid:0.05 in 70
DEG C priming reaction 4h, is then evaporated under reduced pressure 2h, obtains methylvinylcyclosiloxane active catalyst；
(4) long-chain alkyl-silicone oil grafting cyclosiloxane is prepared
By the chain alkyl containing hydrogen silicone oil obtained by t etram-ethyltetravinylcyclotetrasiloxane and step (2) by si-h bond and
Double bond mol ratio is 1.1:1 and platinum content account for gross mass for 0.0006% the step of (3) obtained by ethylene methacrylic basic ring silica
Alkane active catalyst reacts 4h in 100 DEG C, then rises to 180 DEG C of vacuum distillation 4h, obtains the chain alkyl with formula (7) structure
Silicone oil is grafted cyclosiloxane；
(5) organic group modification super high molecular weight polysiloxanes is prepared
By the long-chain alkyl-silicone oil grafting cyclosiloxane and tetramethyl obtained by dimethyl siloxane mixed methylcyclosiloxane, step (4)
The catalyst alkali glue that base ammonium hydroxide content is 1.1% is respectively 100 parts, 20 parts and 0.02 part by mass parts and steamed in 60 DEG C of decompressions
1.5h is evaporated, then adds 0.025 mass parts tetramethyl divinyl disiloxane in 70 DEG C, then rises to 100 DEG C of reaction 1.5h,
Then 180 DEG C of vacuum distillation 6h are risen to, produce the organic group modification super high molecular weight polysiloxanes with formula (1) structure.
Embodiment 3
A kind of preparation method of organic group modification super high molecular weight polysiloxanes, comprises the following steps：
(1) long-chain alpha-olefin activity platinum catalyst is prepared
It is 1 in mass ratio by the aqueous isopropanol of 1- octadecylenes and chloroplatinic acid:0.05, in 75 DEG C of priming reaction 3h, then subtracts
Pressure distillation 2h, obtains long-chain alpha-olefin activity platinum catalyst；
(2) chain alkyl containing hydrogen silicone oil is prepared
It is 1 that containing hydrogen silicone oil and 1- octadecylenes are pressed into si-h bond and double bond mol ratio:1 and platinum content account for gross mass and be
Long-chain alpha-olefin activity platinum catalyst obtained by 0.0002% the step of (1) reacts 4h in 100 DEG C, then rises to 160 DEG C and subtracts
Pressure distillation 2h, obtains the chain alkyl containing hydrogen silicone oil with formula (6) structure；
(3) methylvinylcyclosiloxane active catalyst is prepared
It is 1 in mass ratio by the aqueous isopropanol of t etram-ethyltetravinylcyclotetrasiloxane and chloroplatinic acid:0.05 in 75 DEG C
Priming reaction 3h, is then evaporated under reduced pressure 2h, obtains methylvinylcyclosiloxane active catalyst；
(4) long-chain alkyl-silicone oil grafting cyclosiloxane is prepared
By the chain alkyl containing hydrogen silicone oil obtained by methylvinylcyclosiloxane monomer and step (2) by si-h bond and double
Key mol ratio is 1.1:1 and platinum content account for gross mass for 0.0004% the step of (3) obtained by methylvinylcyclosiloxane
Active catalyst reacts 4h in 100 DEG C, then rises to 180 DEG C of vacuum distillation 4h, obtains the chain alkyl silicon with formula (7) structure
Oil grafting cyclosiloxane；
(5) organic group modification super high molecular weight polysiloxanes is prepared
By the long-chain alkyl-silicone oil grafting cyclosiloxane and tetramethyl hydroxide obtained by cyclosiloxane monomer, step (4)
The catalyst alkali glue that ammonium content is 1.1% is respectively 100 parts, 20 parts and 0.02 part by mass parts and is evaporated under reduced pressure 2h in 55 DEG C, so
0.025 mass parts dimethyl tetravinyl disiloxane is added after 70 DEG C, 100 DEG C of reaction 1h is then risen to, then rises to 180
DEG C be evaporated under reduced pressure 6h, produce the organic group modification super high molecular weight polysiloxanes with formula (1) structure.
Embodiment 4
A kind of preparation method of organic group modification super high molecular weight polysiloxanes, comprises the following steps：
(1) long-chain alpha-olefin activity platinum catalyst is prepared
It is 1 in mass ratio by the aqueous isopropanol of 1- octadecylenes and chloroplatinic acid:0.05, in 75 DEG C of priming reaction 3h, then subtracts
Pressure distillation 2h, obtains long-chain alpha-olefin activity platinum catalyst；
(2) chain alkyl containing hydrogen silicone oil is prepared
It is 1 that containing hydrogen silicone oil and 1- octadecylenes are pressed into si-h bond and double bond mol ratio:1 and platinum content account for gross mass and be
Long-chain alpha-olefin activity platinum catalyst obtained by 0.0002% the step of (1) reacts 4h in 100 DEG C, then rises to 160 DEG C and subtracts
Pressure distillation 2h, obtains the chain alkyl containing hydrogen silicone oil with formula (6) structure；
(3) methylvinylcyclosiloxane active catalyst is prepared
It is 1 in mass ratio by the aqueous isopropanol of t etram-ethyltetravinylcyclotetrasiloxane and chloroplatinic acid:0.05 in 75 DEG C
Priming reaction 3h, is then evaporated under reduced pressure 2h, obtains methylvinylcyclosiloxane active catalyst；
(4) long-chain alkyl-silicone oil grafting cyclosiloxane is prepared
By the chain alkyl containing hydrogen silicone oil obtained by t etram-ethyltetravinylcyclotetrasiloxane and step (2) by si-h bond and
Double bond mol ratio is 1.1:1 and platinum content account for gross mass for 0.0004% the step of (3) obtained by ethylene methacrylic basic ring silica
Alkane active catalyst reacts 4h in 100 DEG C, then rises to 180 DEG C of vacuum distillation 4h, obtains the chain alkyl with formula (7) structure
Silicone oil is grafted cyclosiloxane；
(5) organic group modification super high molecular weight polysiloxanes is prepared
By the long-chain alkyl-silicone oil grafting cyclosiloxane and tetramethyl obtained by dimethyl siloxane mixed methylcyclosiloxane, step (4)
The catalyst alkali glue that base ammonium hydroxide content is 1.1% is respectively 100 parts, 20 parts and 0.02 part by mass parts and steamed in 60 DEG C of decompressions
1.5h is evaporated, then adds 0.025 mass parts dimethyl tetravinyl disiloxane in 70 DEG C, then rises to 100 DEG C of reaction 1.5h,
Then 180 DEG C of vacuum distillation 6h are risen to, produce the organic group modification super high molecular weight polysiloxanes with formula (1) structure.
The embodiment of the present invention is the foregoing is only, but protection scope of the present invention is not limited thereto, this hair
Bright protection domain should be determined by the scope of protection defined in the claims.
Claims (15)
1. a kind of organic group modification super high molecular weight polysiloxanes, it is characterised in that shown in its structural formula such as formula (1)：
In formula (1), a+b sums are the integer more than 12000, and c+d+e sums are 15~250 integer, and f is 6~16 integer,
R is one kind in formula (2), formula (3), formula (4) and formula (5), as follows：
2. a kind of preparation method of organic group modification super high molecular weight polysiloxanes as claimed in claim 1, its feature exist
In comprising the following steps：
(1) long-chain alpha-olefin activity platinum catalyst is prepared
By the alcoholic solution of long-chain alpha-olefin and chloroplatinic acid in 60~80 DEG C of 2~6h of priming reaction, 2~4h is then evaporated under reduced pressure, is obtained
To long-chain alpha-olefin activity platinum catalyst；
(2) chain alkyl containing hydrogen silicone oil is prepared
Long-chain alpha-olefin activity platinum catalyst obtained by step (1) and containing hydrogen silicone oil, long-chain alpha-olefin is anti-in 80~120 DEG C
2~6h is answered, then heats to 140~180 DEG C, 2~4h is evaporated under reduced pressure, obtains the chain alkyl Silicon Containing Hydrogen with formula (6) structure
Oil,
In formula (6), c+d+e sums are 15~250 integer, and f is 6-16 integer；
(3) methylvinylcyclosiloxane activity platinum catalyst is prepared
By the alcoholic solution of methylvinylcyclosiloxane monomer and chloroplatinic acid in 60~80 DEG C of 2~6h of priming reaction, then depressurize
2~4h is distilled, obtains methylvinylcyclosiloxane activity platinum catalyst；
(4) long-chain alkyl-silicone oil grafting cyclosiloxane is prepared
Obtained by the chain alkyl containing hydrogen silicone oil obtained by methylvinylcyclosiloxane monomer, step (2) and step (3)
Methylvinylcyclosiloxane activity platinum catalyst reacts 2~6h in 80~120 DEG C, then rises to 140~180 DEG C of vacuum distillations
2~4h, the long-chain alkyl-silicone oil grafting cyclosiloxane with formula (7) structure is obtained,
In formula (7), c+d+e sums are 15~250 integer, and f is 6~16 integer, and g is 3~5 integer；
(5) organic group modification super high molecular weight polysiloxanes is prepared
By the long-chain alkyl-silicone oil grafting cyclosiloxane obtained by cyclosiloxane monomer, step (4) and catalyst alkali glue in 40~
70 DEG C of 0.5~2h of vacuum distillation, then add unsaturated double-bond end-capping reagent in 60~80 DEG C, then rise to 90~130 DEG C of reactions 1
~4h, 140~220 DEG C of 4~8h of vacuum distillation are then risen to, produce the organic group modification supra polymer with formula (1) structure
Measure polysiloxanes.
3. a kind of preparation method of organic group modification super high molecular weight polysiloxanes as claimed in claim 2, its feature exist
In, long-chain alpha-olefin described in step (1) be 1- octenes, 1- nonenes, 1- decene, 1- hendecenes, 1- laurylenes, 1-tetradecylene,
1- hexadecylenes and 1- octadecylenes one of which or several.
4. a kind of preparation method of organic group modification super high molecular weight polysiloxanes as claimed in claim 2, its feature exist
In the platinum content described in step (1) in the alcoholic solution of chloroplatinic acid is 0.1%, and alcohol used is absolute ethyl alcohol or isopropanol.
5. a kind of preparation method of organic group modification super high molecular weight polysiloxanes as claimed in claim 2, its feature exist
In the mass ratio of the alcoholic solution of long-chain alpha-olefin and chloroplatinic acid described in step (1) is 1:0.01~0.2.
6. a kind of preparation method of organic group modification super high molecular weight polysiloxanes as claimed in claim 2, its feature exist
In the hydrogen content of containing hydrogen silicone oil described in step (2) is 0.1~1.6%.
7. a kind of preparation method of organic group modification super high molecular weight polysiloxanes as claimed in claim 2, its feature exist
In containing hydrogen silicone oil described in step (2) and long-chain alpha-olefin press si-h bond and double bond mol ratio as 1:0.5~1.2 is reacted.
8. a kind of preparation method of organic group modification super high molecular weight polysiloxanes as claimed in claim 2, its feature exist
In, described in step (2) in long-chain alpha-olefin activity platinum catalyst platinum content for containing hydrogen silicone oil, long-chain alpha-olefin and long-chain alpha-
The 0.0001%~0.005% of alkene active platinum catalyst quality summation.
9. a kind of preparation method of organic group modification super high molecular weight polysiloxanes as claimed in claim 2, its feature exist
In methylvinylcyclosiloxane monomer described in step (3) is trimethyl trivinyl cyclotrisiloxane, the ethene of tetramethyl four
One kind in basic ring tetrasiloxane and the vinyl D5 of pentamethyl five.
10. a kind of preparation method of organic group modification super high molecular weight polysiloxanes as claimed in claim 2, its feature exist
In methylvinylcyclosiloxane monomer described in step (4) and chain alkyl containing hydrogen silicone oil press si-h bond and double bond mol ratio
For 1.1~2:1 is reacted.
11. a kind of preparation method of organic group modification super high molecular weight polysiloxanes as claimed in claim 2, its feature exist
In the content of platinum is methylvinylcyclosiloxane in methylvinylcyclosiloxane activity platinum catalyst described in step (4)
Monomer, chain alkyl containing hydrogen silicone oil and methylvinylcyclosiloxane active platinum catalyst quality summation 0.00005%~
0.002%.
12. a kind of preparation method of organic group modification super high molecular weight polysiloxanes as claimed in claim 2, its feature exist
In cyclosiloxane monomer described in step (5) is hexamethyl cyclotrisiloxane, trimethyl triphenyl cyclotrisiloxane, prestox
In cyclotetrasiloxane, tetramethyl tetraphenyl cyclotetrasiloxane, decamethylcyclopentaandoxane and dimethyl siloxane mixed methylcyclosiloxane
It is a kind of.
13. a kind of preparation method of organic group modification super high molecular weight polysiloxanes as claimed in claim 2, its feature exist
In the mass ratio of cyclosiloxane monomer described in step (5) and long-chain alkyl-silicone oil grafting cyclosiloxane is 1:0.01~1.
14. a kind of preparation method of organic group modification super high molecular weight polysiloxanes as claimed in claim 2, its feature exist
In, catalyst alkali glue described in step (5) be cyclosiloxane monomer and TMAH be evaporated under reduced pressure in 50~70 DEG C 4~
Obtained by 8h, wherein the quality of TMAH is cyclosiloxane monomer, long-chain alkyl-silicone oil grafting cyclosiloxane and catalysis
The 0.002%~0.02% of agent alkali glue gross mass.
15. a kind of preparation method of organic group modification super high molecular weight polysiloxanes as claimed in claim 2, its feature exist
In unsaturated double-bond end-capping reagent described in step (5) is dimethyl tetravinyl disiloxane, the silica of tetramethyl divinyl two
One kind in alkane, dimethyl tetraallyl disiloxane and tetramethyl diallyl disiloxane, and its addition is ring silica
Alkane monomer, long-chain alkyl-silicone oil are grafted the 0.01%~0.2% of cyclosiloxane and catalyst alkali colloid amount summation.
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| CN116023666B (en) * | 2023-02-01 | 2023-06-30 | 成都思立可科技有限公司 | Crosslinking agent, silica gel-like TPE and preparation method thereof |
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| CN104927366A (en) * | 2015-06-30 | 2015-09-23 | 广州市斯洛柯高分子聚合物有限公司 | Organic silicon anti-wear agent and preparation method thereof |
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| CN101671436A (en) * | 2009-10-13 | 2010-03-17 | 广州天赐有机硅科技有限公司 | Preparation method for polysiloxane with extra high molecular weight |
| CN104927366A (en) * | 2015-06-30 | 2015-09-23 | 广州市斯洛柯高分子聚合物有限公司 | Organic silicon anti-wear agent and preparation method thereof |
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